CN108356259A - A kind of nanometer of aluminum matrix composite powder and preparation method thereof - Google Patents
A kind of nanometer of aluminum matrix composite powder and preparation method thereof Download PDFInfo
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- CN108356259A CN108356259A CN201810098949.8A CN201810098949A CN108356259A CN 108356259 A CN108356259 A CN 108356259A CN 201810098949 A CN201810098949 A CN 201810098949A CN 108356259 A CN108356259 A CN 108356259A
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- 239000000843 powder Substances 0.000 title claims abstract description 114
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 92
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000002131 composite material Substances 0.000 title claims abstract description 81
- 239000011159 matrix material Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000956 alloy Substances 0.000 claims abstract description 114
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 112
- 239000002245 particle Substances 0.000 claims abstract description 29
- 238000009689 gas atomisation Methods 0.000 claims abstract description 26
- 229910020261 KBF4 Inorganic materials 0.000 claims abstract description 20
- 239000004411 aluminium Substances 0.000 claims abstract description 20
- 229910020491 K2TiF6 Inorganic materials 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 229910033181 TiB2 Inorganic materials 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 229910018507 Al—Ni Inorganic materials 0.000 claims description 19
- 238000012387 aerosolization Methods 0.000 claims description 18
- 229910052719 titanium Inorganic materials 0.000 claims description 18
- 229910018182 Al—Cu Inorganic materials 0.000 claims description 16
- 229910052802 copper Inorganic materials 0.000 claims description 16
- 239000000155 melt Substances 0.000 claims description 16
- 238000007670 refining Methods 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 14
- 229910052727 yttrium Inorganic materials 0.000 claims description 13
- 229910018138 Al-Y Inorganic materials 0.000 claims description 10
- 239000006227 byproduct Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229910018575 Al—Ti Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- 229910052684 Cerium Inorganic materials 0.000 claims description 8
- 229910052706 scandium Inorganic materials 0.000 claims description 8
- 229910018580 Al—Zr Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 38
- 238000010521 absorption reaction Methods 0.000 abstract description 22
- 238000004519 manufacturing process Methods 0.000 abstract description 22
- 238000011065 in-situ storage Methods 0.000 abstract description 15
- 238000005516 engineering process Methods 0.000 abstract description 11
- 239000008187 granular material Substances 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 9
- 229910000838 Al alloy Inorganic materials 0.000 abstract description 8
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract description 3
- 239000005022 packaging material Substances 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 15
- 230000004224 protection Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000004663 powder metallurgy Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000000265 homogenisation Methods 0.000 description 2
- NUHSROFQTUXZQQ-UHFFFAOYSA-N isopentenyl diphosphate Chemical compound CC(=C)CCO[P@](O)(=O)OP(O)(O)=O NUHSROFQTUXZQQ-UHFFFAOYSA-N 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 229910018125 Al-Si Inorganic materials 0.000 description 1
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 1
- 229910018520 Al—Si Inorganic materials 0.000 description 1
- 229910020239 KAlF4 Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- -1 Zr 1%~10% Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/003—Alloys based on aluminium containing at least 2.6% of one or more of the elements: tin, lead, antimony, bismuth, cadmium, and titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0073—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
Abstract
The present invention provides a kind of nanometer of aluminum matrix composite powder and preparation method thereof, preparation method includes：With fine aluminium, pure Ni or Al Ni intermediate alloys, Al Zr intermediate alloys, Al Sc intermediate alloys, Al Cu intermediate alloys, Al Ti intermediate alloys, Al Y intermediate alloys, Al Ce intermediate alloys, KBF4And K2TiF6For raw material, TiB in situ is prepared for using the method that melt-growth in situ controls2Micro-nano granules enhance nanometer aluminum matrix composite, and TiB is prepared by vacuum gas atomization2Particle enhanced aluminum-based composite material powder.The spherical rate ＞ 90% of gained powder, recovery rate >=60%, laser absorption rate>55%.The present invention, which compares traditional Al alloy powder, to be had：(1) for nano particle Dispersed precipitate in matrix grain, thermal stability is more preferable, is suitable for PM technique；(2) have higher laser absorption rate, be more applicable for laser gain material manufacturing technology.
Description
Technical field
The present invention relates to material powder preparing technical fields, and in particular, to a kind of nanometer of aluminum matrix composite powder and
Preparation method.
Background technology
Aerospace, weapons manufacture requirement harshness of the contour leading-edge field to structural material performance and technology of preparing, not only
It is required that while having high-strength high-plasticity, high specific stiffness and specific modulus should also have.The high-end equipment field such as large aircraft
To high-performance, high reliability, pursuit economical and environmentally friendly, cause to large-scale, accurate, the complicated high tough alloy components of integral light
Demand it is more and more urgent.
Laser gain material manufacturing technology can solve to take into account the technology hardly possible that complicated shape and high-performance metal component quickly manufacture
Topic, but commercialized metal powder preparation method such as atomization, rotary electrode method, are limited by the key technologies such as laser absorption rate
The limitation of index, available alloy powder type are limited.Especially in aluminium alloy laser gain material manufacturing field, since aluminium closes
Golden laser absorption rate is relatively low, and only the metal powder of Al-Si alloy systems can be suitable for the field, significantly limit aluminium
Development of the based composites in material increasing field.
Currently, the parts of higher dimensional precision have been prepared using such commercialization powder, and in aerospace, doctor
The fields such as treatment obtain some applications.Such as Boeing companies of the U.S. start since two thousand by LCD large titanium alloy parts
Applied to F-18 and F-22 fighter planes, and the United States Patent (USP) for having applied for airplane parts increasing material manufacturing system in 2015.Europe
AirBus companies begin attempt to undercarriage LCD technology since two thousand six, and by topology optimization design and SLM technology knots
It closes, realizes the optimization manufacture of titanium alloy engine nacelle hinge.GE companies of the U.S. are then walked in SLM technical research and application
Forefront uses the T25 engine sensor shells that SLM technologies manufacture to have been used for GE90-94B aero-engines, and by the U.S.
Federal Aviation Administration ratifies aerospace applications.But the part prepared is also easy to produce the crackle of higher residual stress and micron level
And the defects of hole, and then fatigue of materials intensity, plasticity and toughness is caused to reduce.Thus part production yield rate is low, reliability
Insufficient and cost remains high.Therefore traditional business alloy powder cannot fully meet the manufacture of high-performance components.
Invention content
For the defects in the prior art, the object of the present invention is to provide a kind of nanometer of aluminum matrix composite powder and its systems
Preparation Method, the powder can be provided simultaneously with high laser absorption rate, and high ball form quotient, technological operation is simple and practicable, low-cost high-efficiency, fit
Conjunction is produced in batches.The nano composite powder of preparation is manufactured suitable for laser gain material and powder metallurgy.
To achieve the goals above, a kind of nanometer of aluminum matrix composite powder provided by the invention and preparation method thereof, it is main
The method to be controlled by in-situ authigenic melt, prepares TiB2Particle reinforced aluminum alloy compounding flux recycles autonomous Design
Vacuum aerosolizing device, realize to in-situ self-generated TiB2Prepared by the powder of particle-reinforced aluminum composite material, and then obtain uniformly
The nanometer TiB of Dispersed precipitate2Particle and the equiaxial matrix grain tissue of nanoscale, have prepared the TiB of high laser absorption rate2
Reinforced aluminum matrix composites powder.
The purpose of the present invention is achieved through the following technical solutions：
In a first aspect, it includes base that the present invention, which provides aluminum matrix composite powder described in a kind of nanometer of aluminum matrix composite powder,
Body alloy and the reinforced phase being distributed in described matrix alloy；
Described matrix alloy includes each element component of following mass fraction：Ni 1%~25%；Zr 1%~10%, Cu
0.1%~10%, in Y 0.05%~8%, Sc 0.05%~3%, Ce 0.05%~8% and Ti 0.1%~10% extremely
Few one kind；Al is surplus；
The reinforced phase is TiB2Particle.
Preferably, in described matrix alloy, including Zr 1%~10%, Cu 0.1%~10%, Y 0.05%~8%,
At least two in Sc 0.05%~3%, Ce 0.05%~8% and Ti 0.1%~10%.
Preferably, described matrix alloy includes each element component of following mass fraction：Ni 1%~25%, Zr 1%~
10%, Cu 0.1%~10%, Y 0.05%~8%, Sc 0.05%~3%, Ce 0.05%~8%, Ti 0.1%~
10%, Al are surplus (26%~98%).Cu is a kind of common to carry high performance alloying element；Add micro Sc, Ti element
Can significantly crystal grain thinning, and adding micro Zr elements simultaneously can keep except this advantage, improve material in high temperature
Stability in environment；The moulding and fatigue behaviour of aluminum alloy materials can be improved by adding micro Ce elements；Add micro Y
Element can significantly affect the form of precipitated phase.Therefore, it while adding after Zr, Cu, Y, Sc, Ce, Ti element can improve more preferably
The mechanical property of continuous moulding material.
Preferably, the median particle diameter of the aluminum matrix composite powder is at 3~180 μm；The aluminum matrix composite powder
Middle exist uniformly tiny isometric nanocrystalline, and the isometric nanocrystalline crystallite dimension is 0.1-5 μm.Median particle diameter can reflect
Go out the particle diameter distribution of powder, the bulk density of powder can be directly affected, is one extremely important for laser gain material manufacture
Parameter.Smaller powder grain size is conducive to improve the comprehensive mechanical property of material.
Preferably, it is evenly distributed with TiB in the aluminum matrix composite powder2Particle, the TiB2The size of particle is 5-
2000nm, the TiB2The quality of particle is the 0.5%~10% of aluminum matrix composite powder quality.TiB2Particle size is excessive
The effect of particle strengthening can be cut down, and particle size is too small easily causes reunion.TiB2The mass fraction of particle exceeds above-mentioned model
Enclosing can cause density of material to rise, and toughness significantly reduces, or even spherical powder can not be prepared.
Second aspect, the present invention provide the preparation method of a kind of nanometer of aluminum matrix composite powder, include the following steps：
S1, fine aluminium (commercial-purity aluminium) is heated, heating after coverture covers is added and obtains melt；
S2, by KBF4、K2TiF6Uniformly mixing is added after drying in the melt that step S1 is obtained, mechanical agitation, fully anti-
It answers；(reaction time is generally 5-60min, judges that reaction terminates according to the time.After reaction, it removes and floats on bath surface
Slag, Main By product KAlF4And K3AlF6。)
S3, wait in step S2 after reaction, take out byproduct of reaction, sequentially add pure Ni or Al-Ni intermediate alloys,
In Al-Zr intermediate alloys, Al-Sc intermediate alloys, Al-Cu intermediate alloys, Al-Ti intermediate alloys, Al-Y intermediate alloys and Al-Ce
Between alloy, in the melt be added refining agent carry out refinery by de-gassing, controlled at 650~800 DEG C standing 10~20min, obtain
Aluminum matrix composite melt；
S4, by aluminum matrix composite melt in step S3 by carry out aerosolization, obtain aluminum matrix composite powder (TiB2
Particle enhances nanometer aluminum matrix composite powder)；The aluminum matrix composite powder is subjected to homogenization heat treatment, through screening,
Obtain the aluminum matrix composite powder of suitable dimension (powder size for being suitble to laser gain material manufacture and powder metallurgy).
Preferably, in step S1, the coverture is JZF-03 type high temperature covering agents, is warming up to 600~950 DEG C.It is described
The quality of coverture is the 0.1~1% of fine aluminium quality.
Preferably, in step S2, the KBF4、K2TiF6Mass ratio be 1:0.5~1:2.The KBF4Quality be it is pure
The quality of aluminium is 45~85%%；The churned mechanically rate is 10~500rpm.
Preferably, in step S3, the pure Ni or Al-Ni intermediate alloys, Al-Zr intermediate alloys, Al-Sc intermediate alloys,
Al-Cu intermediate alloys, Al-Ti intermediate alloys, Al-Y intermediate alloys and Al-Ce intermediate alloys addition to meet gained aluminium base multiple
The matrix alloy of condensation material powder includes the elemental constituent of following mass fraction：Ni 1%~25%；Zr 1%~10%, Cu
0.1%~10%, in Y 0.05%~8%, Sc 0.05%~3%, Ce 0.05%~8% and Ti 0.1%~10% extremely
Few one kind.
Preferably, in step S3, Al-Zr intermediate alloys are Al-12wt%Zr, and Al-Ni intermediate alloys are Al-50%Ni,
Al-Sc intermediate alloys are Al-2%Sc, and Al-Cu intermediate alloys are Al-50%Cu, and Al-Ti intermediate alloys are Al-10%Ti, Al-
Y intermediate alloys are Al-30%Y, and Al-Ce intermediate alloys are Al-30%Ce.Alloy uses the order of addition of step S3, if not
It is added in the order described above, by the morphology and size of the second phase in influence system.
Preferably, in step S3, the refining agent is the harmless aluminum refining agent of JZJ types.The quality of the refining agent is
The 0.1~1% of fine aluminium quality.
Preferably, in step S4, the aerosolization condition includes：Solution temperature is 700~1200 DEG C, and aerosolization temperature is
650~1200 DEG C, aerosolization medium is the gaseous mixture of Ar, He or Ar, He, and aerosolization air pressure is 0.5-10MPa.
It need not be heat-treated in the pulverizing process of the present invention.Due to the main function of heat treatment be Homogenization Treatments with
Element segregation is eliminated, aluminum matrix composite powder prepared by the present invention is mainly used for laser gain material manufacture, and laser gain material manufactures
The process to melt again, quickly solidified, therefore heat treatment has little significance to pulverizing process.
The third aspect, the present invention provide a kind of aerosolization of the preparation method for above-mentioned nanometer aluminum matrix composite powder
Device, the gas atomization device include sequentially connected crucible, atomizer, spray chamber and collecting vessel；It is provided in the crucible
Stirring rod, the liquid outlet of the crucible are connected to the nozzle of atomizer；The nozzle of the atomizer is connected to the top of spray chamber,
The lower part of the spray chamber is provided with gas removing pipe, and the gas removing pipe is located at the top of spray chamber and collecting vessel junction；The spray
The diameter 0.5-5mm of mouth.
Nanometer aluminum matrix composite powder prepared by the present invention compares traditional Al alloy powder, (1) nanoscale TiB2Particle
For Dispersed precipitate in matrix grain, thermal stability is more preferable, is suitable for PM technique；(2) have higher laser absorption rate,
It is more applicable for laser gain material manufacturing technology.
Since aluminium alloy laser absorption rate is generally relatively low, great challenge is brought to laser gain material manufacture.What the present invention used
Raw material is the aluminum matrix composite that in-situ authigenic reaction generates, and not only overcomes the outer addition particle surface pollution of tradition, wedge angle is answered
Power concentrates, the deficiencies of interfacial bonding property is poor, and due in pulverizing process cooling velocity quickly, nanoscale TiB2Particle is in matrix
Middle even dispersion distribution, can just play the role of improving powder laser absorptivity.It is influential on laser absorption rate in this system
Mainly Al, Ni and TiB2, wherein laser absorption rate of the laser absorption rate of Al less than 10%, Ni is about 25%, and TiB2Then about
It is 80%, other alloying elements influence little since content is relatively low.Meanwhile in this system, Cu is a kind of common raising performance
Alloying element；Add micro Sc, Ti element can significantly crystal grain thinning, and adding micro Zr elements simultaneously can keep
Except this advantage, the stability of material in the high temperature environment is improved；Aluminum alloy materials can be improved by adding micro Ce elements
Moulding and fatigue behaviour；The form of precipitated phase can be significantly affected by adding micro Y element.In conclusion add simultaneously Zr,
Cu, Y, Sc, Ce, Ti element can more preferably improve the mechanical property of post forming material.
Compared with prior art, the present invention has following advantageous effect：
1, the present invention has been effectively combined the advantage that melt-growth in situ prepares micro-nano particle reinforced.
The aluminum matrix composite powder that micro-nano granules enhancing is prepared by the method for melt-growth in situ, in dispersion composite material
The micro-nano TiB of in-situ authigenic2Particle, while greatly improving the strength of materials, the laser absorption rate of the powder effectively improved, greatly
Width extends the material application range of alumina-base material laser gain material manufacture.
2, the aluminum matrix composite that the present invention is prepared, micro-nano TiB2Particle dispersion is evenly distributed in aluminum substrate,
Have the function of significantly improving laser absorption rate.Meanwhile adding micro at least one of Cu, Zr, Y, Sc, Ce, Ti element
Help to improve the mechanical property of post laser increasing material manufacturing sample.
3, laser gain material manufacture is carried out using the nano composite powder, it is made relative to traditional Al-Si systems powder
Standby strength of materials plasticity is higher, due to nanometer TiB2The humidification of particle and the effect for inhibiting recrystallization growth can be obtained
Uniformly tiny equiax crystal.Due to the micro-nano TiB that even dispersion is distributed in microstructure of composite2Particle and tiny equiax crystal
Presence, the method for the present invention prepare laser gain material manufacture aluminum matrix composite component can have high intensity and high-ductility simultaneously.
4, powder metallurgy forming is carried out using the nano composite powder to be not necessarily to relative to conventional powder metallurgy
Mechanical ball mill is carried out, production cost is greatly reduced.Its structure is nano-scale equiaxed grain structure, and nano particle is uniformly distributed in
In powder matrix, powder metallurgy intensity, plasticity and the modulus of preparation are substantially higher than traditional business aluminium alloy and composite material.
5, the spherical rate ＞ 90% of nanometer aluminum matrix composite powder of the present invention, recovery rate >=60%；The aluminum-base composite
The laser absorption rate of material powder>55%.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the structural schematic diagram of gas atomization device in the present invention；In figure, 1- stirring rod；2- crucibles；3- atomizers；4-
Spray chamber；5- gas removing pipes；6- collecting vessels；
Fig. 2 is the SEM photograph of aluminum matrix composite powder prepared by embodiment 1；Wherein, figure (a) is powder entirety photo,
It is single powder section macrograph to scheme (b).
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, several changes and improvements can also be made.These belong to the present invention
Protection domain.
Embodiment 1
The present embodiment provides a kind of nanometer of aluminum matrix composite powder, preparation method includes：
With fine aluminium, pure Ni or Al-Ni intermediate alloys, Al-12Zr intermediate alloys, Al-Cu intermediate alloys, KBF4And
K2TiF6In-situ authigenic 5wt.%TiB has been prepared for raw material2REINFORCED Al -10Ni-2.3Cu-3Zr composite materials.First high-purity Al is put
Enter and 780 DEG C are melted and be warming up in crucible, is covered with JZF-03 type high temperature covering agents；By KBF4、K2TiF6In mass ratio 1:2
After even mixing, it is added in melt after drying；Wait for after reaction, take out byproduct of reaction, sequentially add Al-Ni intermediate alloys,
Al-12Zr intermediate alloys, Al-Cu intermediate alloys are added the harmless aluminum refining agent of JZJ types and carry out refinery by de-gassing in the melt,
15min is stood at 750 DEG C, then through gas atomization device powder.
The gas atomization device includes sequentially connected crucible 2, atomizer 3, spray chamber 4 and collecting vessel 5；The crucible 2
It is inside provided with stirring rod 1, the liquid outlet of the crucible 2 is connected to the nozzle of atomizer 3；The nozzle of the atomizer 3 and atomization
The top of room 4 is connected to, and the lower part of the spray chamber 4 is provided with gas removing pipe 5, and the gas removing pipe 5 is located at spray chamber 4 and collecting vessel 5
The top of junction.Alloy molten solution in the crucible forms atomized droplet through atomizer in spray chamber, most afterwards through collecting vessel
It is collected.
Gas atomization is：820 DEG C of melt temperature uses He protections and aerosolization, air pressure 2.62MPa, nozzle diameter
2.16mm。
According to GB/T 3249《The assay method of metal and compound powder granularity》, measure 37 μm of powder average diameter；It adopts
It is observed with flying-spot microscope and statistics calculating is carried out using quantitative software for calculation (IPP) after taking pictures, measure powder spherical shape rate ＞
90%；Industry sieve powder obtains required grain size, measures powder yield >=75%；Using GB/T 1482《Metal powder mobility
Assay method》Test mobility is to determine that its mobility meets increasing material manufacturing requirement.Aluminum matrix composite manufactured in the present embodiment
The SEM photograph of powder is as shown in Fig. 2, as can be seen that powder is spherical from Fig. 2 (a)；It can be seen that from Fig. 2 (b)
TiB2Particle is uniformly distributed in the base, and microstructure morphology is in equiax crystal, by quantitative software for calculation (IPP) calculate
It is 460nm to average grain size.With reference to《Physical principle and application of the laser beam with material interaction》, the laser suction of powder
Yield is 61%.
Embodiment 2
The present embodiment provides a kind of nanometer of aluminum matrix composite powder, preparation method includes：
To be closed among fine aluminium, pure Ni or Al-Ni intermediate alloys, Al-12Zr intermediate alloys, Al-Cu intermediate alloys, Al-Ti
Gold, KBF4And K2TiF6In-situ authigenic 5wt.%TiB has been prepared for raw material2REINFORCED Al -10Ni-2.3Cu-3Zr-5Ti is compound
Material.First high-purity Al is put into crucible and melts and be warming up to 780 DEG C, is covered with JZF-03 type high temperature covering agents；By KBF4、
K2TiF6In mass ratio 1:2 after evenly mixing, is added in melt after drying；It waits for after reaction, taking out byproduct of reaction, successively
Al-Ni intermediate alloys, Al-12Zr intermediate alloys, Al-Cu intermediate alloys, Al-Ti intermediate alloys is added, JZJ is added in the melt
The harmless aluminum refining agent of type carries out refinery by de-gassing, 15min is stood at 750 DEG C, then through gas atomization device powder.The gas
Consistent in atomising device and embodiment 1, gas atomization is：900 DEG C of melt temperature uses He protections and aerosolization, air pressure
3.10MPa, nozzle diameter 1.7mm.
15 μm of powder average diameter made from the present embodiment, spherical rate ＞ 90%, recovery rate >=80%, TiB2Granule content
5wt.%, composite powder average grain size 420nm, laser absorption rate 66%.
Embodiment 3
The present embodiment provides a kind of nanometer of aluminum matrix composite powder, preparation method includes：
With fine aluminium, pure Ni or Al-Ni intermediate alloys, Al-Y intermediate alloys, Al-Ce intermediate alloys, KBF4And K2TiF6For
Raw material have prepared in-situ authigenic 10wt.%TiB2REINFORCED Al -15Ni-7Ce-6Y composite materials.High-purity Al is first put into crucible
Middle fusing is simultaneously warming up to 780 DEG C, with the covering of JZF-03 type high temperature covering agents；By KBF4、K2TiF6In mass ratio 1:2 uniformly mixing
Afterwards, it is added in melt after drying；Wait for after reaction, take out byproduct of reaction, sequentially add pure Ni or Al-Ni intermediate alloys,
Al-Y intermediate alloys, Al-Ce intermediate alloys are added the harmless aluminum refining agent of JZJ types and carry out refinery by de-gassing in the melt,
15min is stood at 750 DEG C, then through gas atomization device powder.The gas atomization device and consistent in embodiment 1, aerosolization
Technique is：900 DEG C of melt temperature uses Ar protections and aerosolization, air pressure 1.20MPa, nozzle diameter 2.16mm.
45 μm of powder average diameter made from the present embodiment, spherical rate ＞ 90%, recovery rate >=75%, TiB2Granule content
10wt.%, composite powder average grain size 530nm, laser absorption rate 62%.
Embodiment 4
The present embodiment provides a kind of nanometer of aluminum matrix composite powder, preparation method includes：
To be closed among fine aluminium, pure Ni or Al-Ni intermediate alloys, Al-12Zr intermediate alloys, Al-Sc intermediate alloys, Al-Cu
Gold, Al-Ce intermediate alloys, KBF4And K2TiF6In-situ authigenic 10wt.%TiB has been prepared for raw material2REINFORCED Al -16Ni-
2.2Cu-0.7Ce-9Zr-1Sc composite material.First high-purity Al is put into crucible and melts and be warming up to 780 DEG C, with JZF-03 types
High temperature covering agent covers；By KBF4、K2TiF6In mass ratio 1:2 after evenly mixing, is added in melt after drying；To the end of reaction
Afterwards, byproduct of reaction is taken out, adds pure Ni or Al-Ni intermediate alloys, Al-12Zr intermediate alloys, Al-Sc intermediate alloys, Al- successively
Cu intermediate alloys, Al-Ce intermediate alloys are added the harmless aluminum refining agent of JZJ types and carry out refinery by de-gassing, in the melt 750
15min is stood at DEG C, then through gas atomization device powder.The gas atomization device and consistent in embodiment 1, gas atomization
For：900 DEG C of melt temperature uses Ar protections and aerosolization, air pressure 5.10MPa, nozzle diameter 2.16mm.
27 μm of powder average diameter made from the present embodiment, spherical rate ＞ 90%, recovery rate >=60%, TiB2Granule content
10wt.%, composite powder average grain size 512nm, laser absorption rate 67%.
Embodiment 5
The present embodiment provides a kind of nanometer of aluminum matrix composite powder, preparation method includes：
To be closed among fine aluminium, pure Ni or Al-Ni intermediate alloys, Al-12Zr intermediate alloys, Al-Cu intermediate alloys, Al-Y
Gold, KBF4And K2TiF6In-situ authigenic 8wt.%TiB has been prepared for raw material2REINFORCED Al -6Ni-8Cu-4Zr-4Y composite materials.
First high-purity Al is put into crucible and melts and be warming up to 780 DEG C, is covered with JZF-03 type high temperature covering agents；By KBF4、K2TiF6It presses
Mass ratio 1:2 after evenly mixing, is added in melt after drying；It waits for after reaction, taking out byproduct of reaction, sequentially adding Al-
Al-12Zr intermediate alloys, Al-Cu intermediate alloys, Al-Y intermediate alloys, the harmless aluminium of JZJ types is added in Ni intermediate alloys in the melt
Alloy refining agent carries out refinery by de-gassing, 15min is stood at 750 DEG C, then through gas atomization device powder.The gas atomization device
With it is consistent in embodiment 1, gas atomization is：900 DEG C of melt temperature, uses 50%Ar and 50%He mixing gas shielded and gas
Atomization, air pressure 3.10MPa, nozzle diameter 1.7mm.
22 μm of powder average diameter made from the present embodiment, spherical rate ＞ 90%, recovery rate >=60%, TiB2Granule content
8wt.%, composite powder average grain size 480nm, laser absorption rate 59%.
Embodiment 6
The present embodiment provides a kind of nanometer of aluminum matrix composite powder, preparation method includes：
With fine aluminium, pure Ni or Al-Ni intermediate alloys, Al-Zr intermediate alloys, Al-Sc intermediate alloys, Al-Cu intermediate alloys,
Al-Ti intermediate alloys, Al-Y intermediate alloys, Al-Ce intermediate alloys, KBF4And K2TiF6In-situ authigenic has been prepared for raw material
5wt.%TiB2REINFORCED Al -6Ni-2.2Cu-0.7Ce-9Zr-1Sc-1Ti-6Y composite materials.First high-purity Al is put into crucible
It melts and is warming up to 780 DEG C, with the covering of JZF-03 type high temperature covering agents；By KBF4、K2TiF6In mass ratio 1:2 after evenly mixing,
It is added in melt after drying；It waits for after reaction, taking out byproduct of reaction, sequentially adding pure Ni or Al-Ni intermediate alloys, Al-
Among Zr intermediate alloys, Al-Sc intermediate alloys, Al-Cu intermediate alloys, Al-Ti intermediate alloys, Al-Y intermediate alloys and Al-Ce
Alloy is added the harmless aluminum refining agent of JZJ types and carries out refinery by de-gassing, 15min is stood at 750 DEG C, is then passed through in the melt
Gas atomization device powder.Consistent in the gas atomization device and embodiment 1, gas atomization is：900 DEG C of melt temperature, makes
With Ar protections and aerosolization, air pressure 5.10MPa, nozzle diameter 2.16mm.
24 μm of powder average diameter made from the present embodiment, spherical rate ＞ 90%, recovery rate >=60%, TiB2Granule content
5wt.%, composite powder average grain size 446nm, laser absorption rate 55%.
Embodiment 7
The present embodiment provides a kind of nanometer of aluminum matrix composite powder, preparation method includes：
With fine aluminium, pure Ni or Al-Ni intermediate alloys, Al-Cu intermediate alloys, KBF4And K2TiF6It is prepared for raw material
In-situ authigenic 5wt.%TiB2REINFORCED Al -10Ni-2.3Cu composite materials.First high-purity Al is put into crucible and melts and is warming up to
It 780 DEG C, is covered with JZF-03 type high temperature covering agents；By KBF4、K2TiF6In mass ratio 1:2 after evenly mixing, is added after drying molten
In body；It waits for after reaction, taking out byproduct of reaction, sequentially adding Al-Ni intermediate alloys, Al-Cu intermediate alloys, in the melt
The harmless aluminum refining agent of JZJ types is added and carries out refinery by de-gassing, 15min is stood at 750 DEG C, then through gas atomization device system
Powder.Consistent in the gas atomization device and embodiment 1, gas atomization is：Gas atomization is：850 DEG C of melt temperature, makes
With He protections and aerosolization, air pressure 2.68MPa, nozzle diameter 2.2mm.
38 μm of powder average diameter made from the present embodiment, spherical rate ＞ 90%, recovery rate >=60%, TiB2Granule content
5wt.%, 4.7 μm of composite powder average grain size, laser absorption rate 55%.
Nanometer aluminum matrix composite powder prepared by above-described embodiment 1-7, not only powder property is excellent, but also is subsequently testing
Found in card effect, when adding the powder prepared by least two elements in Zr, Cu, Y, Sc, Ce, Ti, than only add Zr,
The powder prepared by a kind of element in Cu, Y, Sc, Ce, Ti has preferable when being manufactured sample for laser gain material
Mechanical property.Moreover, the powder for adding Zr, Cu, Y, Sc, Ce and Ti element simultaneously can more preferably improve the power of post forming material
Performance is learned, molding sample obtained has best comprehensive mechanical property.
Comparative example 1
This comparative example is related to a kind of nanometer of aluminum matrix composite powder, and preparation method and embodiment 1 are almost the same, different
Place is：Al-Ni intermediate alloys are replaced using technical pure Zn and technical pure Mg intermediate alloys, obtain Al-7Zn-3Mg-
2.3Cu-3Zr composite material.
32 μm of powder average diameter made from this comparative example, spherical rate ＞ 90%, recovery rate >=60%, TiB2Granule content
5wt.%, 1.8 μm of composite powder average grain size, laser absorption rate 37%.
To sum up, the nanometer aluminum matrix composite powder that prepared by the present invention, micro-nano TiB2Particle dispersion is evenly distributed on aluminium
In matrix, have the function of significantly improving laser absorption rate；Add at least one in micro Cu, Zr, Y, Sc, Ce, Ti element
Kind helps to improve the mechanical property of post laser increasing material manufacturing sample.And the powder of Zr, Cu, Y, Sc, Ce, Ti element is added simultaneously
End can more preferably improve the mechanical property of post forming material,
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make a variety of changes or change within the scope of the claims, this not shadow
Ring the substantive content of the present invention.In the absence of conflict, the feature in embodiments herein and embodiment can arbitrary phase
Mutually combination.
Claims (10)
1. a kind of nanometer of aluminum matrix composite powder, which is characterized in that the aluminum matrix composite powder include matrix alloy and
The reinforced phase being distributed in described matrix alloy；
Described matrix alloy includes each element component of following mass fraction：Ni 1%~25%；Zr 1%~10%, Cu
0.1%~10%, in Y 0.05%~8%, Sc 0.05%~3%, Ce 0.05%~8% and Ti 0.1%~10% extremely
Few one kind；Al is surplus；
The reinforced phase is TiB2Particle.
2. according to claim 1 nanometer of aluminum matrix composite powder, which is characterized in that described matrix alloy includes as follows
The each element component of mass fraction：Ni 1%~25%, Zr 1%~10%, Cu 0.1%~10%, Y 0.05%~8%,
Sc 0.05%~3%, Ce 0.05%~8%, Ti 0.1%~10%, Al are surplus.
3. according to claim 1 or 2 nanometer of aluminum matrix composite powder, which is characterized in that the aluminum matrix composite
The median particle diameter of powder is at 3~180 μm；Exist in the aluminum matrix composite powder it is uniformly tiny isometric nanocrystalline, it is described
Isometric nanocrystalline crystallite dimension is 0.1-5 μm.
4. according to claim 1 or 2 nanometer of aluminum matrix composite powder, which is characterized in that the TiB2Particle uniformly divides
Cloth is in described matrix alloy, the TiB2The size of particle is 5-2000nm；The TiB2The quality of particle is aluminum-base composite material
Expect the 0.5%~10% of powder quality.
5. a kind of preparation method of nanometer aluminum matrix composite powder according to claim 1, which is characterized in that including such as
Lower step：
S1, fine aluminium is heated, heating after coverture covers is added and obtains melt；
S2, by KBF4、K2TiF6Uniformly mixing is added after drying in the melt that step S1 is obtained, mechanical agitation, fully reacts；
S3, it waits in step S2 after reaction, taking out byproduct of reaction, sequentially adding pure Ni or Al-Ni intermediate alloys, Al-Zr
It is closed among intermediate alloy, Al-Sc intermediate alloys, Al-Cu intermediate alloys, Al-Ti intermediate alloys, Al-Y intermediate alloys and Al-Ce
Gold is added refining agent and carries out refinery by de-gassing in the melt, controlled at 650~800 DEG C of 10~20min of standing, obtains aluminium base
Composite Melt；
S4, the aluminum matrix composite melt for obtaining step S3 carry out aerosolization, obtain aluminum matrix composite powder；Through screening,
Obtain the aluminum matrix composite powder of suitable dimension.
6. the preparation method of according to claim 5 nanometer of aluminum matrix composite powder, which is characterized in that in step S1,
The coverture is JZF-03 type high temperature covering agents, is warming up to 600~950 DEG C.
7. the preparation method of according to claim 5 nanometer of aluminum matrix composite powder, which is characterized in that in step S2,
The KBF4、K2TiF6Mass ratio be 1:0.5~1:2.
8. the preparation method of according to claim 5 nanometer of aluminum matrix composite powder, which is characterized in that in step S3,
The pure Ni or Al-Ni intermediate alloys, Al-Zr intermediate alloys, Al-Sc intermediate alloys, Al-Cu intermediate alloys, the centres Al-Ti are closed
Gold, Al-Y intermediate alloys and Al-Ce intermediate alloys addition meet the matrix alloy of gained aluminum matrix composite powder and include
The elemental constituent of following mass fraction：Ni 1%~25%；Zr 1%~10%, Cu 0.1%~10%, Y 0.05%~
8%, at least one of Sc 0.05%~3%, Ce 0.05%~8% and Ti 0.1%~10%；
The refining agent is the harmless aluminum refining agent of JZJ types.
9. the preparation method of according to claim 5 nanometer of aluminum matrix composite powder, which is characterized in that in step S4,
The aerosolization condition includes：Melt temperature is 700~1200 DEG C, and aerosolization temperature is 650~1200 DEG C, and aerosolization medium is
The gaseous mixture of Ar, He or Ar, He, aerosolization air pressure are 0.5-10MPa.
10. a kind of gas atomization device of preparation method for the nanometer aluminum matrix composite powder described in claim 5, special
Sign is that the gas atomization device includes sequentially connected crucible, atomizer, spray chamber and collecting vessel；Setting in the crucible
There are stirring rod, the liquid outlet of the crucible to be connected to the nozzle of atomizer；The nozzle of the atomizer and the top of spray chamber connect
Logical, the lower part of the spray chamber is provided with gas removing pipe, and the gas removing pipe is located at the top of spray chamber and collecting vessel junction；It is described
The diameter 0.5-5mm of nozzle.
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| CN109593994A (en) * | 2019-01-28 | 2019-04-09 | 兰州理工大学 | Add the method that Rare-Earth Ce element reduces aluminum matrix composite hot cracking tendency |
| CN109692964A (en) * | 2019-01-31 | 2019-04-30 | 中南大学 | A kind of reinforced aluminum matrix composites and preparation method thereof |
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| CN115430843A (en) * | 2022-08-16 | 2022-12-06 | 上海交通大学 | Double-phase particle reinforced additive aluminum alloy and preparation method thereof |
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